CN102060540A - Method for preparing Re:YAG polycrystalline transparent ceramic by using different molding modes - Google Patents
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Abstract
The invention relates to a method for preparing Re:YAG polycrystalline transparent ceramic by using different molding modes, which adopts commercial high-purity Y2O3, Al2O3 and Re2O3 as raw materials, adopts MgO, CaO or TEOS (tetraethyl orthosilicate) as sintering additive, and prepares a raw blank by a cold isostatic pressing, slip casting or tape casting process to react and sinter the transparent polycrystalline Re:YAG ceramic. The method comprises the following steps: mixing and adding the oxides into a liquid medium; adding a certain amount of dispersant, adhesive, plasticizer, pressing agent and defoaming agent, carrying out ball milling, and mixing; treating the slurry under different conditions in different molding modes to obtain the raw blank; and sintering the degreased raw blank in a vacuum furnace. For the Re:YAG ceramic sintering body with thickness of 1.5mm, the transmission rate of straight light in the wavelength of 1064nm is not lower than 80% after the Re:YAG ceramic sintering body is subjected to double-sided polishing. For the raw blank which is prepared by different molding modes and is sintered for 10 hours at 1750 DEG C, sizes of ceramic grains are different, wherein regarding the raw blank prepared by cold isostatic pressing, the average grain of the ceramic is 13.5mu m; regarding the raw blank prepared by slip casting, the average grain of the ceramic is 3.5mu m; and regarding the raw blank prepared by tape casting, the average grain of the ceramic is 1.5mu m.
Description
Technical field
The invention provides the method that several different molding modes prepare the Re:YAG polycrystalline transparent ceramic, belong to special optical ceramic process technical field.
Background technology
Traditional laser host material is monocrystalline or glass normally, and the YAG monocrystalline is most important a kind of Solid State Laser substrate material, mixes Nd
3+, Er
3+, Ho
3+, Tm
3+, Yb
3+, Cr
3+Deng rare earth or transition group ionic YAG monocrystalline all is the laser crystals of excellent property, and they are widely used in many fields such as scientific research, environmental protection, laser medicine, laser processings.But, owing to be subjected to single crystal growing technology limitation, crystalline size and doping content all to be difficult to improve.Single crystal growing needs the precious metal crucible in addition, and growth cycle is long, so cost is higher, so scientists expects to find a kind of novel method of the YAG of preparation laser host material always.Nineteen ninety-five, people [the Ikesue.A such as scientist A.Ikesue of Japan, Kinoshita.T, Kamata.K, et al. " Fabrication optical properties ofhigh-performance polycrystalline Nd:YAG ceramics for solid-statelasers ", J.Am.Ceram.Soc., 78 (4) (1995): 1033-1040] use TEOS as sintering agent, with the Al of sub-micron grade
2O
3, Y
2O
3And Nd
2O
3Be raw material, adopt cold isostatic compaction, prepare high transparent Nd:YAG pottery first, obtain laser output first, but laser power and efficient are not high in conjunction with vacuum sintering technology.A kind of urea coprecipitation method that this advances of Japanese subsequently Konoshima chemical company's employing is prepared high sintering activity powder [Jpn Patent 10-101333.1998-04-21, Jpn Patent10-101411.1998-04-21], adopt the injection forming technology to prepare high transparent Nd:YAG pottery [JpnPatent 10-67555.1998-03-10], and the laser of having realized Nd:YAG laser ceramics 1.46kW is exported [Jianren Lu, Ken-ichi Ueda, Hideki Yagi, et al. " Neodymium doped yttrium alaminum garnet (Y3Al5O12) nanocrystalline ceramics-a new generation of solidstate laser and optical materials ", Journal of Alloys and Compounds., 341 (2002) 220-225].
From top example we as can be seen forming method the sintering of pottery and the last transparency are had significant effects, the green compact quality of moulding has determined the optical quality of sintered ceramic.The traditional ceramics molding mode is fit to the molding mode of laser ceramics as dry-pressing formed, cold isostatic compaction, injection forming, flow casting molding etc.Cold isostatic compaction green density height, burn till shrink little, not yielding, but require initial powder granule good fluidity, the almost spherical of moulding, if the green compact of the of poor quality very difficult preparation even structure of powder are difficult to whole even, the measured ceramic body of matter of sintering; The green structure of injection forming evenly, pore UNICOM, this eliminating that helps little pore in the vacuum sintering process obtains even structure, density height, ceramic that optical quality is good, and prepares large-sized sample easily; The flow casting molding mode is applicable to the gradient material of preparation different levels of doping, and the moulding green structure is even, plasticity good, be easy to processing, can prepare green compact thickness 0.6～1.5mm, width 0.6～1.2m large size thin slice sample.
The present invention is that the oxide powder with commercialization is a raw material, adopt quiet moulding, injection forming, these several molding modes of flow casting molding such as cold, each parameter in the control moulding process, prepare high-quality moulding green compact, prepare high transparent Re:YAG pottery through vacuum sintering, and compare these several molding modes to preparing the relative merits of Re:YAG laser ceramics, domestic genus reported first.Raw material of the present invention does not need special, but commercially available commercial powder, raw materials cost reduces, and experimental repeatability is good, is the operational path that a kind of suitability for industrialized is produced.
Summary of the invention
The objective of the invention is to utilize different molding modes to prepare the Re:YAG polycrystalline transparent ceramic in conjunction with vacuum sintering, the sintered compact of transparent polycrystalline oxide ceramics is represented that by general formula R e:YAG Re is Nd, Yb, Cr, Er, Ce, Sm, Eu, Ho, Tm, a kind of in the Pr rare earth element or several, this method is characterized in that technical process is followed successively by: the preparation of different molding mode Re:YAG ceramic sizes, froth in vacuum, moulding, the demoulding, drying, binder removal, burn till.The concrete following steps of implementing:
(1) according to Re
xY
3-xAl
5O
12Commercially available purity 〉=the 99.99%Y of stoichiometric ratio weighing of (x is the material molar weight that part Re atom replaces the Y atom, O＜x≤0.1) molecular formula
2O
3Powder 0.0297～0.0288mol, purity 〉=99.99%Al
2O
3Powder 0.025mol, purity 〉=99.99%Nd
2O
3Powder 0.0003～0012mol; Add a certain proportion of dispersion agent, binding agent, softening agent, defrother, die mould agent, sintering aid (MgO, TEOS or CaO) by dry powder weight; The addition of sintering aid MgO is 0～2at% of the mole amount of mixed powder, and the TEOS addition is 0～2wt% of mixed powder weight, and the CaO sintering aid is 0～2wt% of mixed powder weight.
(2) mix solution by a certain percentage as the ball milling liquid medium with in deionized water, alcohols, acetone, benzene, the dimethylbenzene one or more, carry out batch mixing by abrading-ball and ball mill, by weight expecting: ball: liquid medium=1: (1～20): (1～20);
Quiet moulding dispersion agent additions such as (3) different molding mode wet end furnishs are inconsistent, and are cold are dry powder quality 0.05～1wt%, content of binder 0.5～5wt%, die mould agent addition 0.1～2wt%; Add the dispersion agent of relative dry powder weight 0.1wt%～5wt%, 0.1wt～5wt% binding agent, 0.2～10wt% softening agent, 0.1～5wt% defrother for injection forming; Slurry dispersion agent addition for flow casting molding is 0.01～1wt% with respect to dry powder weight, content of binder 1～20wt%, softening agent addition 2～15wt%, defrother addition 0.5～5wt%.Powder, dispersion agent, binding agent, softening agent, die mould agent, defrother mixing and ball milling.For isostatic pressing slurry dispersion agent is oleic acid, Viscotrol C, polyacrylate, and binding agent is polyvinyl butyral (PVB), polyvinyl alcohol (PVA), and the die mould agent is unsaturated fatty acids, butyl stearate, octyl stearate; The kind of adding dispersion agent for the slurry of injection forming is a polyelectrolyte class dispersion agent, the non-ionic polyalcohol dispersion agent, high price small molecules class dispersion agent, binding agent can adopt polyvinyl alcohol (PVA), polyvinyl butyral acetal (PVB), polyvinyl acetate, methylcellulose gum, carboxymethyl cellulose, ethyl cellulose, Natvosol, hydroxypropylcellulose, polyoxyethylene, ethene one vinyl acetate copolymer, softening agent can adopt different molecular weight polyethylene glycol, and defrother can adopt organic polar form compound; Slurry dispersion agent for flow casting molding is menhaden fish oil, fish oil, and binding agent is polyvinyl butyral (PVB), and softening agent is phthalic acid fourth Bian ester (BBP), BBP dibutyl phthalate (DBP), polyalkylene glycol (PAG), and defrother is an octanol.
(4) molding procedure is taked different modes at different moulding processs, cold isostatic compaction is with the mixed slurry of ball milling, in baking oven, ground 200 mesh sieves after 80 ℃ of dryings, powder is filled in the rubber mold, put into cold isostatic press behind the Vacuum Package mould at 100～300Mpa forming under the pressure, injection forming and flow casting molding are that the slurry that ball milling mixes is stirred de-bubble under vacuum or little negative pressure, do not have in slurry till the bubble effusion; Slurry after the de-bubble injects gypsum mold, treats that gypsum mold suction slurry finishes, and base substrate shrinks and separates with gypsum mold, sloughs mould; The de-bubble disposed slurry injects the casting machine hopper, evenly spreads upon by scraper on the film band of uniform rotation, and base plate is heated to the base substrate that is fit in the temperature baked film band;
(5) green compact after the moulding are put into alumina crucible, and crucible and sample are packed in the vacuum oven, and 0.1～10 ℃/min of heat-up rate is warming up to organism decomposition temperature point at a slow speed, and size insulation per sample is 0.2h～100h.Can utilize vacuum degreasing, oxygen atmosphere protection degreasing, nitrogen atmosphere protection degreasing or the degreasing of protection of inert gas atmosphere;
(6) green compact after the degreasing are put into vacuum oven, carry out sintering under vacuum atmosphere, 1500 ℃～1900 ℃ of sintering ranges, and size per sample, sintering time is 0.5～100 hour.
Description of drawings
Fig. 1 is the photo in kind of Nd:YAG ceramics sample.The diagram sample is that different molding modes prepare green compact (from left to right being cold isostatic compaction successively, injection forming, flow casting molding) at 1750 ℃ of sintering after 10 hours, the annealing 20 hours down of 1450 ℃ of oxygen atmospheres, and twin polishing is to the photo of the thick sample of 1.5mm;
Fig. 2 is the XRD crystalline phase analysis of the Nd:YAG ceramics sample of 1750 ℃ of sintering after 10 hours, and the diffraction peak among the figure does not have middle transition phase YAP, YAM to occur all corresponding to a cube YAG crystalline phase as seen from the figure, has shown that the oxide compound in the raw material reacts completely;
Fig. 3 is the straight line transmittance curve of different ceramics samples, and the straight line transmitance is followed successively by 81.5%, 83.3%, 83.6% at laser emission wavelength 1064nm place;
Fig. 4 obtains Nd:YAG for different molding modes prepare green compact (from left to right being cold isostatic compaction successively, injection forming, flow casting molding) at 1750 ℃ of sintering after 10 hours, at 2 hours ceramic crystalline grain scanning electron microscope (SEM) of 1500 ℃ of thermal etchings figure.
Embodiment
Embodiment 1:
α-Al2O3Fen body with 5.098g, 6.7066g the Y2O3 powder, 0.1010g Nd2O3,0.0600g TEOS and 0.0600g Viscotrol C, 0.3600g PVB, the 0.1200g unsaturated fatty acids is put into high-purity agate jar, adds high-purity agate ball of 72g, 11.800g dehydrated alcohol, mixing and ball milling 24h.Behind the ball milling that slurry is dry in 80 ℃ of baking ovens, to put into agate mortar after dry 48 hours and grind, powder is crossed 200 mesh sieves.With the forcing spindle of 2～10Mpa to unidirectional pressurization, the disk of compression moulding Φ 15, cold isostatic compaction under the pressure of 200Mpa again.The green compact of isostatic pressing are put into tube furnace be warmed up to 700 ℃ with 1 ℃/min temperature rise rate under oxygen atmosphere, be incubated 2 hours, oxygen flow is per minute 50～100ml, and insulation finishes naturally cooling.Green compact after the degreasing are put into vacuum oven, are 1.5 * 10 in vacuum tightness
-4Carry out sintering under the Pa air pressure, be raised to 1200 ℃ with 10 ℃/min temperature rise rate, then with 5 ℃/min temperature rise rate be warming up to 1750 ℃ and 1750 ℃ the insulation 10 hours, drop to 1200 ℃ with 3 ℃/min rate of temperature fall, naturally cool to room temperature.Obtain transparent Nd:YAG pottery.Ceramics sample was annealed 20 hours under 1450 ℃ of oxygen atmospheres, with surface grinding machine and the husky lapping paste of Buddha's warrior attendant pottery was carried out mirror ultrafinish, and it is thick to be ground to 1.50mm.Left side photo is the photo in kind of polishing back 1at%Nd:YAG pottery among Fig. 1, from XRD diffracting spectrum (1 diffraction peak Fig. 2) as can be seen this ceramics sample be pure phase YAG and do not have dephasign YAP, the YAM of transition, record with the UV, visible light near infrared spectrometer that to locate the straight line transmitance in optical maser wavelength (1064nm) be 81.5% (1 curve among Fig. 3).Under 1500 ℃ of air atmospheres, this sample was carried out thermal etching 2 hours,, find that median size is 13.5 μ m (left side figure among Fig. 4) by scanning electron microscope (SEM) observation sample microtexture.Determine its median size with SEM etc. by the line that on the full resolution pricture of sample, draws arbitrarily.When the length of line is C, the numbers of particles on this line is N, and when ratio of enlargement was M, median size formula: median size=1.56C/ (MN) asked.
By the commercially available high-purity powder of stoichiometric ratio weighing: Y
2O
3: 10.0600g, Al
2O
3: 7.6470g, Nd
2O
3: 0.1516g, the MgO sintering aid of interpolation 0.5at%, 0.2wt% dispersion agent poly carboxylic acid, 0.2wt% binding agent polyvinyl alcohol, 0.5wt% defrother propyl carbinol; Raw material, abrading-ball, ball milling additive are poured into 100 gram deionized water ball millings mixed rotational speed of ball-mill 350r/m, material: ball=1: 10 12 hours.The mixed slurry of ball milling is put into vacuum tank, and vacuum-treat to vacuum tightness reaches-below the 0.1Mpa, does not have in the slurry till the bubble effusion; Slurry after the de-bubble injects gypsum mold, treats that gypsum mold suction slurry finishes, and base substrate shrinks and separates with gypsum mold, sloughs mould.The green compact of moulding dry in the shade for some time in room temperature earlier, put into baking oven again from 30 ℃ of insulations 5 hours, and 40 ℃ are incubated 3 hours, and 60 ℃ are incubated 2 hours, slowly are raised to 100 ℃ of branch gradient dried.Other process such as embodiment 1, ceramics sample was annealed 20 hours under 1450 ℃ of oxygen atmospheres, twin polishing is to 1.5mm thick (Fig. 1 intermediate photograph), what X-ray diffraction analysis XRD figure spectrum recorded this ceramics sample is pure YAG phase mutually, do not have middle transition phase YAP, YAM to occur, shown the oxide compound in the raw material react completely (2 diffraction peaks among Fig. 2); Recording in 1064nm wavelength place straight line transmitance by the UV, visible light near infrared spectrometer is 83.3% (2 curves among Fig. 3).Under 1500 ℃ of air atmospheres, this sample was carried out thermal etching 2 hours,, find that median size is 3.5 μ m (Fig. 4 middle graph) by scanning electron microscope (SEM) observation sample microtexture.
By the commercially available high-purity powder of stoichiometric ratio weighing: Y
2O
3: 10.0600g, Al
2O
3: 7.6470g, Nd
2O
3: 0.1516g, add the MgO sintering aid of 0.5at%, add 0.06wt% dispersion agent fish oil, raw material is added to 60 grams by in dehydrated alcohol and the dimethylbenzene mixed solvent, material: ball=1: 5, ball milling mixed 5～24 hours, afterwards adding 10wt% binding agent polyvinyl butyral in the slurry that mixes, the 5wt% softening agent is phthalic acid fourth Bian ester and 1wt% polyalkylene glycol, 0.5wt% defrother octanol remix ball milling 5～24 hours.The mixed slurry of ball milling is put into the froth in vacuum machine, and under negative pressure, being stirred to does not have in the slurry till the bubble effusion.Slurry after the de-bubble is poured in the hopper of casting machine, opens mechanical motor, and uniform rotation film band evenly spreads upon on the film band by scraper, and base plate is heated to and is fit to temperature drying forming base substrate, and base substrate separates with the film band.The good green compact of drying be cut into 20mm * 20mm square folded thick put into to be pressurized under 100 ℃ of the static pressure press such as temperature take out sample after being incubated 20 minutes 50Mpa pressure under, obtain the thick base substrate of 2～4mm, other process such as embodiment 1.The Nd:YAG ceramics sample that obtains was annealed 20 hours under 1450 ℃ of oxygen atmospheres, twin polishing is to 1.5mm thick (the right photo among Fig. 1), what X-ray diffraction analysis XRD figure spectrum recorded this ceramics sample is pure YAG phase mutually, do not have middle transition phase YAP, YAM to occur, shown the oxide compound in the raw material react completely (3 diffraction peaks among Fig. 2); Recording in 1064nm wavelength place straight line transmitance by the UV, visible light near infrared spectrometer is 83.6% (3 curves among Fig. 3).Under 1500 ℃ of air atmospheres, this sample was carried out thermal etching 2 hours,, find that median size is 1.5 μ m (the right figure among Fig. 4) by scanning electron microscope (SEM) observation sample microtexture.
Claims (10)
1. utilize different molding modes to prepare the method for Re:YAG polycrystalline transparent ceramic, it is characterized in that technical process is followed successively by: the preparation of different molding mode Re:YAG ceramic sizes, froth in vacuum, moulding, the demoulding, drying, binder removal, burn till.
2. utilize different molding modes to prepare the method for Re:YAG polycrystalline transparent ceramic as claim 1, it is characterized in that, molding mode is that compact density is higher than 50%, the molding mode that contaminating impurity is few.
3. the method for preparing the Re:YAG polycrystalline transparent ceramic as claimed in claim 2 is characterized in that, molding mode is cold isostatic compaction, injection forming or flow casting molding.
4. utilize different molding modes to prepare the method for Re:YAG polycrystalline transparent ceramic as claim 3, it is characterized in that the used slurry of cold isostatic compaction, injection forming or flow casting molding is according to Re
xY
3-xAl
5O
12, wherein x is the material molar weight that part Re atom replaces the Y atom, the array mode of 0＜x≤0.1 molecular formula is by the Y of molecular formula stoichiometric ratio weighing purity 〉=99.99%
2O
3Powder, the Al of purity 〉=99.99%
2O
3Powder, the Re of purity 〉=99.99%
2O
3Powder; Interpolation is with respect to a certain proportion of dispersion agent of dry powder weight, binding agent, softening agent, defrother, die mould agent, sintering aid, and ball milling mixes.
5. the different molding modes of utilization as claimed in claim 4 prepare the method for Re:YAG polycrystalline transparent ceramic, it is characterized in that the ball milling solvent is that used liquid medium is made up of deionized water, alcohols, acetone, benzene, dimethylbenzene, or mix mixing and ball milling 0.5～100 hour by a certain percentage by wherein several.
6. the different molding modes of utilization as claimed in claim 5 prepare the method for Re:YAG polycrystalline transparent ceramic, after it is characterized in that ball milling mixing disposed slurry drying and screening, cold isostatic compaction base substrate under the pressure of 100～300Mpa, according to big or small dwell time of green compact be 1～10min.
7. the different molding modes of utilization as claimed in claim 5 prepare the method for Re:YAG polycrystalline transparent ceramic, it is characterized in that the mixed slurry of ball milling, vacuum-treat to vacuum tightness reaches-below the 0.1Mpa or little negative pressure, till not having bubble to overflow in slurry, the slurry after the de-bubble injects the gypsum mold molding blank.
8. the different molding modes of utilization as claimed in claim 5 prepare the method for Re:YAG polycrystalline transparent ceramic, it is characterized in that the slurry after the de-bubble, pour in the casting machine hopper, evenly spread upon on the film band of uniform rotation base plate heating, drying molding blank by scraper.
9. the different molding modes of utilization as claimed in claim 5 prepare the method for Re:YAG polycrystalline transparent ceramic, it is characterized in that the dispersion agent that different molding mode slurries is added, binding agent, softening agent, the die mould agent, the ratio of defrother is different with kind: quiet moulding dispersion agent oleic acid such as cold, Viscotrol C or polyacrylate addition are dry powder quality 0.05～1wt%, polyvinyl butyral or polyvinyl alcohol adhesive addition are dry powder quality 0.5～5wt%, die mould agent unsaturated fatty acids, butyl stearate or octyl stearate addition are dry powder quality 0.1～2wt%; Add the polyelectrolyte class dispersion agent of relative dry powder weight 0.1wt%～5wt% for injection forming, non-ionic polyalcohol dispersion agent or high price small molecules class are as dispersion agent, add relative dry powder weight 0.1wt～5wt% polyvinyl alcohol, polyvinyl butyral acetal, polyvinyl acetate, methylcellulose gum, carboxymethyl cellulose, ethyl cellulose, Natvosol, hydroxypropylcellulose, polyoxyethylene, ethene one vinyl acetate copolymer is wherein a kind of or several are as binding agent, add relative dry powder weight 0.2～10wt% polyoxyethylene glycol as softening agent, add the organic polar form compound of relative dry powder weight 0.1～5wt% as defrother; Slurry interpolation for flow casting molding is 0.01～1wt% dispersion agent menhaden fish oil, fish oil or KD1 with respect to dry powder weight, interpolation is 1～20wt% binding agent polyvinyl butyral acetal with respect to dry powder weight, interpolation is added with respect to dry powder weight 0.5～5wt% defrother octanol with respect to dry powder weight 2～15wt% plasticizer phthalic acid fourth Bian ester, dibutyl phthalate or polyalkylene glycol;
10. the different molding modes of utilization as claimed in claim 5 prepare the method for Re:YAG polycrystalline transparent ceramic, it is characterized in that this preparation method also comprises: the addition of sintering aid MgO is 0～2at% of the mole amount of mixed powder, the TEOS addition is 0～2wt% of mixed powder weight, and the CaO sintering aid is 0～2wt% of mixed powder weight; The degreasing under vacuum degreasing, oxygen atmosphere protection degreasing, nitrogen atmosphere protection degreasing or protection of inert gas atmosphere of the green compact of moulding; Carry out sintering under vacuum or hydrogen atmosphere, sintering temperature is not less than 1500 ℃ not high 1900 ℃, and sintering time is more than at least 0.5 hour.
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